CN110900925A - Preparation method of PEEK with topological pattern on surface - Google Patents

Preparation method of PEEK with topological pattern on surface Download PDF

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Publication number
CN110900925A
CN110900925A CN201911181631.7A CN201911181631A CN110900925A CN 110900925 A CN110900925 A CN 110900925A CN 201911181631 A CN201911181631 A CN 201911181631A CN 110900925 A CN110900925 A CN 110900925A
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China
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peek
template
topological pattern
topological
temperature
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Chinese (zh)
Inventor
任富增
朱明余
黄金财
王晓飞
何进
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Southwest University of Science and Technology
Southern University of Science and Technology
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Southwest University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
    • B29C43/021—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles characterised by the shape of the surface
    • B29C2043/023—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles characterised by the shape of the surface having a plurality of grooves
    • B29C2043/025—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles characterised by the shape of the surface having a plurality of grooves forming a microstructure, i.e. fine patterning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • B29C2043/5808—Measuring, controlling or regulating pressure or compressing force
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • B29C2043/5816—Measuring, controlling or regulating temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2071/00—Use of polyethers, e.g. PEEK, i.e. polyether-etherketone or PEK, i.e. polyetherketone or derivatives thereof, as moulding material

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention provides a preparation method of PEEK with topological patterns on the surface. The preparation method comprises the following steps: (1) the PEEK material is placed on a template with a topological pattern on the surface, the PEEK material is pressed and molded by a cold pressing method, a hot pressing method or a method of firstly cold pressing and then heating, and the topological pattern on the template is transferred to the surface of the pressed and molded PEEK; (2) and separating the template from the PEEK subjected to compression molding to obtain the PEEK with the topological pattern on the surface. The method provided by the invention can form the self-designed topological pattern on the surface of the PEEK in a large area, the formed topological pattern has higher resolution, and the elastic modulus of the patterned PEEK can be adjusted by adjusting the extrusion molding condition so as to adapt to different application requirements.

Description

Preparation method of PEEK with topological pattern on surface
Technical Field
The invention belongs to the technical field of medical implant materials, and particularly relates to a preparation method of PEEK with topological patterns on the surface.
Background
Titanium and titanium alloys have been the traditional choice for bone implant materials by virtue of good physicochemical properties, mechanical properties, fatigue resistance and corrosion resistance. However, the elastic modulus of titanium is much higher than that of compact bone of human body (titanium is 110GPa, and compact bone is only 14GPa), and the difference directly produces stress shielding effect, so that the periphery of the compact bone bears little stress, and the bone shrinkage and bone absorption of the bone around the implant are caused. In addition, studies have shown that titanium implants cause allergic reactions in vivo. Much research is currently devoted to finding alternative materials for conventional titanium bone implants.
In the last 90 s of the century, PEEK (polyetheretherketone) has received extensive attention due to its excellent chemical stability and corrosion resistance, in particular its elastic modulus matching human bone, and is used as a long-term implant. However, the surface characteristics of the implant, including surface roughness, wettability and chemical composition, are important factors in controlling the interaction of the cells with the substrate. The hydrophobic nature of the PEEK surface results in poor cell adhesion and poor osteointegration. For this reason, researchers have explored methods for surface modification, including plasma treatment, laser treatment, and wet chemistry methods.
The plasma treatment technique utilizes non-polymerizable gases (e.g., Ar, N)2，CO、NH3、O2、H2Etc.) plasma gas interacts with the polymer surface to form new functional groups on the surface to improve wettability, adhesion and biocompatibility. CN103881129A discloses a method for performing plasma immersion ion implantation on the surface of a polyetheretherketone material by using argon as an ion source, and then soaking the polyetheretherketone material subjected to the plasma immersion ion implantation in a hydrogen peroxide aqueous solution. The surface of the modified polyetheretherketone material has a nano structure with shallow holes. Researches show that the regular topological structure can effectively improve the surface physicochemical property of the material and induce cell differentiation. However, a regular topological structure cannot be formed on the surface of PEEK through ultraviolet irradiation or plasma treatment.
CN 108503877A discloses that a sulfonated group is formed on the surface of PEEK by using sulfuric acid and reduction treatment is carried out by using sodium borohydride by using a wet chemical method, so that a micron topological structure can be effectively formed on the surface of PEEK and good hydrophilicity is achieved. However, this method cannot form a regular topological pattern, and is environmentally unfriendly and requires a long modification time.
The laser treatment can change the surface characteristics of the material, and form a regular pattern on the surface of the hard material, thereby increasing the wettability and the cell adhesion of the hard material. However, the laser-machined pattern shapes are typically larger than the size of a single cell, making it difficult to build micron topologies close to the cell size.
At present, the surface modification of the PEEK implant is mainly focused on improving the surface characteristics of the PEEK implant by using methods such as plasma etching, film deposition, sand blasting and the like. These methods, however, do not allow for controlled changes in the PEEK surface structure or surface microtopography with a variety of self-designs. Laser processing can cause the PEEK surface to be seriously melted, and a regular pattern is difficult to maintain; and due to the limitation of the size of the laser beam, the pattern resolution is not high, the pattern requirement of submicron scale cannot be met, and large-scale surface patterning cannot be realized at the same time.
Therefore, development of a PEEK surface modification method capable of changing the surface structure in a large scale, high precision, controllable manner or designing diversified surface micro topology by oneself is required.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of PEEK with topological patterns on the surface. Compared with the existing method, the preparation method provided by the invention can form the self-designed topological pattern on the surface of the PEEK, can realize large-scale patterning of the surface of the PEEK, improves the resolution of the topological pattern, and can adjust the elastic modulus of the patterned PEEK according to the application requirement.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of PEEK with topological patterns on the surface, which comprises the following steps:
(1) the PEEK material is placed on a template with a topological pattern on the surface, the PEEK material is pressed and molded by a cold pressing method, a hot pressing method or a method of firstly cold pressing and then heating, and the topological pattern on the template is transferred to the surface of the pressed and molded PEEK;
(2) and separating the template from the PEEK subjected to compression molding to obtain the PEEK with the topological pattern on the surface.
A process method for constructing an expected topological structure on the surface of medical PEEK rapidly and in high precision and large area is still blank. According to the invention, the PEEK material is subjected to cold pressing and hot pressing or cold pressing and heating on the template with the topological pattern on the surface, so that the rapid, high-precision and large-area topological structure can be constructed on the PEEK surface. The topological structure can be designed into any patterns such as grooves, cylindrical bulges, stripes and the like by changing the topological pattern on the template. The prepared PEEK with the surface having the topological pattern can effectively guide cell growth, increase cell adhesion and accelerate cell differentiation.
In a preferred embodiment of the present invention, the PEEK material in step (1) is a PEEK block, a PEEK film, or a PEEK powder, preferably a PEEK powder.
When the PEEK powder is selected as the raw material, the pore structure of the molded PEEK can be adjusted by controlling the extrusion molding condition, and the modulus of the PEEK can be adjusted, so that different application requirements can be met. For example, when the molded PEEK is used as an orthopedic implant material, the modulus can be adjusted to match that of human cancellous bone.
As a preferred technical scheme of the invention, the material of the template is metal.
Preferably, the material of the template is titanium, tantalum or iron, and further preferably titanium.
As a preferred embodiment of the present invention, the method for forming the topological pattern on the template comprises: lithography combined with inductively coupled plasma etching, lithography combined with deep reactive ion etching, electrochemical etching, or laser direct writing.
As a preferred embodiment of the present invention, the temperature of the cold pressing in the step (1) is 10 to 30 ℃ and may be, for example, 10 ℃, 12 ℃, 13 ℃, 15 ℃, 16 ℃, 18 ℃, 19 ℃, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 28 ℃ or 30 ℃ or the like; the pressure is 50 to 1000MPa, and may be, for example, 50MPa, 60MPa, 80MPa, 100MPa, 150MPa, 200MPa, 250MPa, 300MPa, 350MPa, 400MPa, 450MPa, 500MPa, 550MPa, 600MPa, 650MPa, 700MPa, 750MPa, 800MPa, 850MPa, 900MPa, 950MPa or 1000 MPa.
Preferably, the temperature of the cold pressing in the step (1) is 10-30 ℃, and the pressure is 400-800 MPa.
As the preferred embodiment of the present invention, the hot pressing temperature in step (1) is 50-350 ℃, for example, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 120 ℃, 130 ℃, 150 ℃, 160 ℃, 180 ℃, 200 ℃, 220 ℃, 230 ℃, 250 ℃, 260 ℃, 280 ℃, 300 ℃, 320 ℃, 330 ℃ or 350 ℃ and the like; the pressure is 50 to 1000MPa, and may be, for example, 50MPa, 60MPa, 80MPa, 100MPa, 150MPa, 200MPa, 250MPa, 300MPa, 350MPa, 400MPa, 450MPa, 500MPa, 550MPa, 600MPa, 650MPa, 700MPa, 750MPa, 800MPa, 850MPa, 900MPa, 950MPa or 1000 MPa.
Preferably, the temperature of the hot pressing in the step (1) is 150-.
As a preferred embodiment of the present invention, in the step (1), the cold pressing temperature for the cold pressing and then heating is 10 to 30 ℃, and may be, for example, 10 ℃, 12 ℃, 13 ℃, 15 ℃, 16 ℃, 18 ℃, 19 ℃, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 28 ℃ or 30 ℃ or the like; the cold pressing pressure is 50 to 1000MPa, and may be, for example, 50MPa, 60MPa, 80MPa, 100MPa, 150MPa, 200MPa, 250MPa, 300MPa, 350MPa, 400MPa, 450MPa, 500MPa, 550MPa, 600MPa, 650MPa, 700MPa, 750MPa, 800MPa, 850MPa, 900MPa, 950MPa, 1000MPa, or the like; the heating temperature is 50-350 deg.C, such as 50 deg.C, 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, 100 deg.C, 120 deg.C, 130 deg.C, 150 deg.C, 160 deg.C, 180 deg.C, 200 deg.C, 220 deg.C, 230 deg.C, 250 deg.C, 260 deg.C, 280 deg.C, 300 deg.C, 320 deg..
Preferably, in the step (1), the cold pressing temperature after the cold pressing and the heating is 10-30 ℃, the cold pressing pressure is 400-800MPa, and the heating temperature is 150-280 ℃.
The extrusion molding method of cold pressing followed by heating may cause some degree of deformation of PEEK during heating, causing a decrease in resolution of the topology pattern formed on PEEK, and thus the cold or hot pressing forming method is more preferable in the present invention.
As a preferable technical scheme of the invention, the pressurizing time in the step (1) is 1-3 min; for example, it may be 1min, 1.2min, 1.5min, 1.8min, 2min, 2.2min, 2.5min, 2.8min or 3 min.
As the preferred technical scheme of the invention, the elastic modulus of the PEEK with the topological pattern on the surface is 0.01-3 GPa; for example, the amount of the component may be 0.01GPa, 002GPa, 0.05GPa, 0.08GPa, 0.1GPa, 0.2GPa, 0.3GPa, 0.4GPa, 0.5GPa, 0.6GPa, 0.7GPa, 0.8GPa, 0.9GPa, 1GPa, 1.2GPa, 1.5GPa, 1.8GPa, 2GPa, 2.2GPa, 2.5GPa, 2.8GPa or 3GPa, etc.
The elastic modulus range of the human cancellous bone is 0.01-3Gpa, and the elastic modulus of the prepared PEEK with the surface having the topological pattern is controlled within the range, so that the PEEK and the PEEK can be matched with each other, and the repair of the cancellous bone is promoted.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) preparing a topological pattern on the surface of a titanium substrate by utilizing photoetching combined with inductively coupled plasma etching (ICP), photoetching combined with deep Reactive Ion Etching (RIE), electrochemical etching or laser direct writing to obtain a template with the surface having the topological pattern;
(2) placing PEEK powder on the template with the surface provided with the topological pattern obtained in the step (1), cold-pressing for 1-3min under the conditions that the temperature is 10-30 ℃ and the pressure is 400-800MPa, or hot-pressing for 1-3min under the conditions that the temperature is 150-280 ℃ and the pressure is 400-800MPa, and carrying out compression molding on the PEEK powder, and simultaneously transferring the topological pattern on the template to the surface of the compression-molded PEEK;
(3) and mechanically separating the template from the PEEK subjected to compression molding to obtain the PEEK with the topological pattern on the surface.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the PEEK with the topological patterns on the surface can adopt powder, film or block PEEK to be molded in one step, is simple to operate and environment-friendly, can prepare the topological patterns in a large area, can control the formed topological appearance, can design different topological appearances according to requirements to guide cell growth, increases the cell adherence rate, has higher resolution, and overcomes the defects of low laser surface modification resolution and uncontrollable topological structures formed by plasma treatment and wet chemical methods. In addition, the preparation method provided by the invention can adjust the elastic modulus of the patterned PEEK by adjusting the extrusion molding conditions so as to adapt to different application requirements. The preparation method provided by the invention is a novel PEEK surface modification method, and has good application prospect in the field of preparation of orthopedic and dental implant materials.
Drawings
FIG. 1 is a scanning electron micrograph of a PEEK surface topology provided in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a PEEK surface topology provided in example 2 of the present invention;
FIG. 3 is a scanning electron micrograph of a PEEK surface topology provided in example 3 of the present invention;
FIG. 4 is a scanning electron micrograph of a PEEK surface topology provided in example 5 of the present invention;
FIG. 5 is a scanning electron micrograph of a PEEK surface topology provided in example 6 of the present invention;
FIG. 6 is a scanning electron micrograph of a PEEK surface topology provided in example 7 of the present invention;
fig. 7 is a scanning electron micrograph of the PEEK surface topology provided in embodiment 8 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It should be understood by those skilled in the art that the specific embodiments are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The raw materials used in the examples of the invention are as follows:
PEEK powder: mreda, USA (800 mesh, Cat No: M045941);
PEEK film: wuhan Jiejiangsheng science and technology Limited (Cat. No. 2-9240-06).
Example 1
The embodiment provides a preparation method of PEEK with topological patterns on the surface, which comprises the following steps:
(1) preparing a topological pattern on the surface of a titanium substrate by utilizing photoetching combined with ICP (inductively coupled plasma) to obtain a template with the surface provided with the topological pattern;
(2) placing PEEK powder on the template with the surface provided with the topological pattern obtained in the step (1), cold-pressing for 3min at the temperature of 22 ℃ and under the pressure of 100MPa, and carrying out compression molding on the PEEK powder, and simultaneously transferring the topological pattern on the template to the surface of the compression-molded PEEK;
(3) and separating the template from the PEEK subjected to compression molding by using mechanical force to obtain the PEEK with the topological pattern on the surface.
According to GB/T22315-. The surface morphology of PEEK provided in this example was observed using a scanning electron microscope, and the results are shown in fig. 1. As can be seen from fig. 1, the topology structure of the PEEK surface is clear, but since the molding pressure is small, the PEEK structure is loose and has many voids.
Example 2
This example provides a method for preparing PEEK having a topological pattern on the surface, which is different from example 1 in that the cold pressing pressure in step (2) is 400 MPa.
According to GB/T22315-. The surface morphology of PEEK provided in this example was observed using a scanning electron microscope, and the results are shown in fig. 2. As can be seen from fig. 2, the present example provides a PEEK surface with a clear topology and a denser structure than example 1.
Example 3
This example provides a method for preparing PEEK having a topological pattern on the surface, which is different from example 1 in that the cold pressing pressure in step (2) is 600MPa, and the topological pattern is different.
According to GB/T22315-. The surface morphology of PEEK provided in this example was observed using a scanning electron microscope, and the results are shown in fig. 3. As can be seen from fig. 3, the present example provides a PEEK surface with a clear topology and a denser structure than example 1.
Example 4
The embodiment provides a preparation method of PEEK with topological patterns on the surface, which comprises the following steps:
(1) preparing a topological pattern on the surface of the titanium substrate by utilizing photoetching combined with RIE to obtain a template with the surface having the topological pattern;
(2) placing PEEK powder on the template with the surface provided with the topological pattern obtained in the step (1), cold-pressing for 3min at the temperature of 22 ℃ and under the pressure of 100MPa, and carrying out compression molding on the PEEK powder, and simultaneously transferring the topological pattern on the template to the surface of the compression-molded PEEK;
(3) and separating the template from the PEEK subjected to compression molding by using mechanical force to obtain the PEEK with the topological pattern on the surface.
According to GB/T22315-.
Example 5
The embodiment provides a preparation method of PEEK with topological patterns on the surface, which comprises the following steps:
(1) preparing a topological pattern on the surface of a titanium substrate by utilizing photoetching combined with ICP (inductively coupled plasma) to obtain a template with the surface provided with the topological pattern;
(2) placing PEEK powder on the template with the surface provided with the topological pattern obtained in the step (1), cold-pressing for 3min at the temperature of 22 ℃ and the pressure of 400MPa, carrying out compression molding on the PEEK powder, and then carrying out heat treatment for 1h at the temperature of 300 ℃ to transfer the topological pattern on the template to the surface of the compression-molded PEEK;
(3) and separating the template from the PEEK subjected to compression molding by using mechanical force to obtain the PEEK with the topological pattern on the surface.
According to GB/T22315-. The surface morphology of PEEK provided in this example was observed using a scanning electron microscope, and the results are shown in fig. 4. As can be seen from fig. 4, the topology of the PEEK surface provided in this example is clear, but the resolution is reduced compared to example 2.
Example 6
The embodiment provides a preparation method of PEEK with topological patterns on the surface, which comprises the following steps:
(1) preparing a topological pattern on the surface of a titanium substrate by utilizing photoetching combined with ICP (inductively coupled plasma) to obtain a template with the surface provided with the topological pattern;
(2) placing the PEEK film on the template with the topological pattern on the surface obtained in the step (1), hot-pressing for 3min at the temperature of 200 ℃ and the pressure of 400MPa, and performing compression molding on the PEEK film, and simultaneously transferring the topological pattern on the template to the surface of the compression-molded PEEK;
(3) and separating the template from the PEEK subjected to compression molding by using mechanical force to obtain the PEEK with the topological pattern on the surface.
According to GB/T22315-. The surface morphology of PEEK provided in this example was observed using a scanning electron microscope, and the results are shown in fig. 5. As can be seen from FIG. 5, the PEEK provided by the present example has a dense structure and a clear surface topology.
Example 7
This example provides a method for preparing PEEK with a topological pattern on its surface, which is different from example 6 in that the hot pressing conditions in step (2) are as follows: hot pressing at 50 deg.C and 1000MPa for 2 min.
According to GB/T22315-. The surface morphology of PEEK provided in this example was observed using a scanning electron microscope, and the results are shown in fig. 6. As can be seen from fig. 6, the PEEK structure provided by this example is dense and the topology of the surface is clear.
Example 8
This example provides a method for preparing PEEK with a topological pattern on its surface, which is different from example 6 in that the hot pressing conditions in step (2) are as follows: hot pressing at 350 deg.C and 50MPa for 1 min.
According to GB/T22315-. The surface morphology of PEEK provided in this example was observed using a scanning electron microscope, and the results are shown in fig. 7. As can be seen from fig. 7, the PEEK structure provided by this example is dense and the topology of the surface is clear.
Example 9
This example provides a method for preparing PEEK with a topological pattern on its surface, which is different from example 6 in that the hot pressing conditions in step (2) are as follows: hot pressing at 150 deg.C and 800MPa for 3 min.
According to GB/T22315-.
Example 10
This example provides a method for preparing PEEK with a topological pattern on its surface, which is different from example 6 in that the hot pressing conditions in step (2) are as follows: hot pressing at 280 deg.C and 600MPa for 1.5 min.
According to GB/T22315-.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. A preparation method of PEEK with topological patterns on the surface is characterized by comprising the following steps:
(1) the PEEK material is placed on a template with a topological pattern on the surface, the PEEK material is pressed and molded by a cold pressing method, a hot pressing method or a method of firstly cold pressing and then heating, and the topological pattern on the template is transferred to the surface of the pressed and molded PEEK;
(2) and separating the template from the PEEK subjected to compression molding to obtain the PEEK with the topological pattern on the surface.
2. The method according to claim 1, wherein the PEEK material in step (1) is a PEEK block, a PEEK film or a PEEK powder, preferably a PEEK powder.
3. The production method according to claim 1 or 2, wherein a material of the template is a metal;
preferably, the material of the template is titanium, tantalum or iron, and further preferably titanium.
4. The method for preparing according to any one of claims 1 to 3, wherein the topological pattern on the template is formed by: lithography combined with inductively coupled plasma etching, lithography combined with deep reactive ion etching, electrochemical etching, or laser direct writing.
5. The process according to any one of claims 1 to 4, wherein the cold pressing in step (1) is carried out at a temperature of 10 to 30 ℃ and a pressure of 50 to 1000 MPa;
preferably, the temperature of the cold pressing in the step (1) is 10-30 ℃, and the pressure is 400-800 MPa.
6. The production method according to any one of claims 1 to 5, wherein the temperature of the hot pressing in the step (1) is 50 to 350 ℃, and the pressure is 50 to 1000 MPa;
preferably, the temperature of the hot pressing in the step (1) is 150-.
7. The preparation method according to any one of claims 1 to 6, wherein the cold pressing temperature of the step (1) of cold pressing and heating is 10 to 30 ℃, the cold pressing pressure is 50 to 1000MPa, and the heating temperature is 50 to 350 ℃;
preferably, in the step (1), the cold pressing temperature after the cold pressing and the heating is 10-30 ℃, the cold pressing pressure is 400-800MPa, and the heating temperature is 150-280 ℃.
8. The production method according to any one of claims 1 to 7, wherein the pressurization time in the step (1) is 1 to 3 min.
9. The production method according to any one of claims 1 to 8, wherein the PEEK having the surface with the topological pattern has an elastic modulus of 0.01 to 3 GPa.
10. The production method according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) preparing a topological pattern on the surface of a titanium substrate by utilizing photoetching combined with inductively coupled plasma etching, photoetching combined with deep reactive ion etching, electrochemical etching or laser direct writing to obtain a template with the surface provided with the topological pattern;
(2) placing PEEK powder on the template with the surface provided with the topological pattern obtained in the step (1), cold-pressing for 1-3min under the conditions that the temperature is 10-30 ℃ and the pressure is 400-800MPa, or hot-pressing for 1-3min under the conditions that the temperature is 150-280 ℃ and the pressure is 400-800MPa, and carrying out compression molding on the PEEK powder, and simultaneously transferring the topological pattern on the template to the surface of the compression-molded PEEK;
(3) and mechanically separating the template from the PEEK subjected to compression molding to obtain the PEEK with the topological pattern on the surface.
CN201911181631.7A 2019-11-27 2019-11-27 Preparation method of PEEK with topological pattern on surface Pending CN110900925A (en)

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